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Al-X / AlOx / Al junctions
Al-X / AlOx / Al junctionsEdit

    samples done on 2013-072014-112014-12, 2015-01

    table to note probe station measurements (find pdf to print at the bottom of this page)
    4 probes Junction A (=top) Junction B Junction C Junction D (bottom)
    1-2 5-6:  (-value short) 3-4:  1-2:  16-15: 
    3-4 7-8:  9-10:  11-12:  14-13: 
    1-3 5-7:  3-9:  1-11:  16-14: 
    1-4 5-8:  3-10:  1-12:  16-13: 
    2-3 6-7:  4-9:  2-11:  15-14: 
    2-4 6-8:  4-10:  2-12:  15-13: 
    size (nm x nm)        

     

    Results: Double oxidation on old evaporator

    All values from 10/2014 were on a linear slope, then suddenly went down by a factor ~2 since 12/2014.
    Initial / final means before and after any treatment (ashing, heating, observation, etc)
    All tests were 5 minutes. Only pressure was varied. The 'dose'=P*t is given for real O2 pressure (15% of the abs pressure).
    Reproducibility issues are thought to come from (STILL TO DEBUG)
    - bad gauge in the <100mb range ?
    - series junctions on chip ?
    - bad lithography (resist residues which affect the junction resistance) ?
    - evolution of the Ar/O2 bottle content ?

    double-oxi_odl-evap.jpg

    established procedure n°2:
    large area contacts are done with e-beam

    step 1: bilayer

    When spin on full wafer:

    - spin MAA8.5 EL10 (batch , exp. ) @ 2000rpm for 60"
    - bake hot plate setpoint 180°C, 5'
    - spin PMMA A6 (batch , exp. ) @ 6000rpm for 60"
    - bake hot plate setpoint 180°C, 15'

    The thickness was measured with two techniques:

    First, we define lines with SEM, develop, cleave, sputter and observe under angle
    Tihs gives the following values (statistics on 5 - 6 samples, with 30 lines on each)
    Drawback: the resist is modified by the SEM observation, even though it is sputtered, and we make fast images.
    MAA = 530 +/- 20nm
    PMMA = 240 +/- 20nm

    Second, we infer the bilayer thickness from double angle displacement (first evaep @ 0°, second evap at 35° for instance). With a statistic over 4 samples, with 4 patterns on each, we obtain:
    Drawback: the mask is closing with the first evaporation. The mask might be lifted up or down.
    MAA = 670 +/- 60nm
    PMMA =  +/- nm

    When spin on single 5x5mm chip:

    - spin MAA8.5 EL10 (batch , exp. ) @ 2000rpm for 45" + 10" @ 8000rpm (acc. 4000rpm/s)
    - bake hot plate setpoint 180°C, 5'
    - spin PMMA A6 (batch , exp. ) @ 5000rpm for 45" + 10" @ 8000rpm (acc. 4000rpm/s)
    - bake hot plate setpoint 180°C, 15'

    comparable thicknesses, relatively more uniform spin than with standard recipe.
    Measured on one sample, at ellipsometer,
    MAA = 660nm
    PMMA = 320nm @ 4000rpm (no measure @ 5k or 6k)

    step 2: exposure

    Precise exposure pattern was quite long to optimize.
    GUIDELINES:

    • Have a sufficient dose for the connections. Standard dose = 300µC/cm2 for 30keV

    spot 1: dose x 1.4 (in position list)
    spot 4: dose x 1.2 (in position list)
    spot 7: dose x 1.8
     (in position list). This compensates for drift in current along exposure. Do critical patterns first (ie alignement cross, or small arms)

    • Have a large overlap between patterns

    on x2000 field, overlap is at least 
    between x2000 spot 1 and x1000 spot 4, overlap is 
    between x1000 spot 4 and x32 spot 7, overlap (tolerance) is 3µm

    Note there is significant proximity effect of large connecting areas onto the small patterns (eg the undercuts), over few µms.
     

    step 3: development

    Development will affect the subsequent resist residues and undercut.
    Although no recipe has been shown to really impede resist residues, we found that rinsing using a mix of ethanol and IPA (1:1) increases the undercut, which might also reduce the residual resist atomic layer on the substrate.

    No comparative measurements were done on the undercuts. (TODO)

    dev: MIBK - IPA (1:3) 1'
    rinse: IPA - ethanol (1:1) 1'
    rinse 2: IPA 15"

    step 4: evaporation
    - ion mill 3mA 500V, 20" @ 0°
    optional - Ti pump ([email protected]/s on backside of holder) -> P_ch = 4e-8
    - Al 30nm @ 1nm/s, 0°, P_ev = mb
    - ox 5'@ XXXmb
    ( when double oxidation is required
    - Al 0.6nm @ 0.1nm/s, 0° (note each time the actual value at shutter close)
    - ox 5' @ XXXmb
    )
    optional - Ti pump -> P_ch = 8e-8
    - Al 60nm @ 1nm/s, +35°, P_ev = 4e-7mb

    This 0° / +35° with the above bilayer gives ~550nm displacement (from top of bilayer), and 450nm displacement including masking by the PMMA hanging mask (so from bottom of PMMA).
    This indicates: 785nm total thickness, 640nm MAA thickness

    Note when using 40° angle, one has 600nm displacement from top of bilayer, 500nm from bottom of PMMA. 
    -> 600nm MAA, 715nm total

    step 5: lift-off

    Warm (65°C) PG remover for about 30 minutes.
    NO ULTRA SOUND! Use pipette to finish lift.
    Rinse ODI

    step 6: junction stabilization to ageing
    • Asher O2, 2' @ 100W, 200µb to remove resist residues and stabilize junctions resistances.
      Effect is systematic increase by about 10% after ashing
    • 1 min @ 100°C on hot plate.
      Effect is to lower dispersion on junctions values, and is typically similar to asher (increase by 10%)

     

    step 7: probe station measurement

    Preferably use 4W measurements that are more accurate. The leads are typically 60ohm each.
    Fill the table below with measurements

    4 probes Junction A (=top) Junction B Junction C Junction D (bottom)
    Rpol (Ohm) 1M 10k 1M 1M 1M
    V (mV) 14.28 111.94 13.39 11.92 16.31 14.65 14.49 12.93
    I (µA) 5.04 481.1 5.04 4.99 5.04 4.99 5.04 4.99
    Rj (Ohm) 2833.3 232.7 2656.7 2388.7 3236.1 2935.9 2875 2591.2
    overlap 158 x 1020 164 x 1090 158 x 893 160 x 980
    Ohm*um2 456.6 37.5 474.9 427.0 456.6 414.2 451 406.3

    left: after SEM observation
    right: + ozone plasma 2', 200µb, 100W
    red: got shunted

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    Fichiers 10

    FichierTailleDateAttaché par 
     2014-10_OxyQuantro.xlsx Modifier
    partial summary of oxidation at SPEC
    42.29 Ko01:20, 28 Jan 2015Helene_Le_SueurActions
     2016_oxidation.opj
    Aucune description
    819.58 Ko17:36, 13 Jul 2016Helene_Le_SueurActions
     ChloeR_grid100n_600nmPMGI-250nmPMMA_+-20deg_30-60nm.PNG
    Chloe works on quartz or glass. She does ion milling in situ (ashing?)
    10.26 Ko11:49, 6 Nov 2014Helene_Le_SueurActions
    double-oxi_odl-evap.jpg
    earliest points 2014-10 showed higher resistances, then from 12/2014 all went down to ~half the value
    219.63 Ko22:51, 21 Jan 2015Helene_Le_SueurActions
     fiche-mesures-tunnel.pdf
    Aucune description
    24.05 Ko13:02, 27 Jan 2016Helene_Le_SueurActions
     fiche-mesures-tunnel.svg
    Aucune description
    148.32 Ko13:02, 27 Jan 2016Helene_Le_SueurActions
     junctions.nb
    Aucune description
    21.85 Ko11:01, 15 Jan 2015Helene_Le_SueurActions
     oxidation.opj
    Aucune description
    369.71 Ko22:34, 21 Jan 2015Helene_Le_SueurActions
     VSbefore04-2014_grid100n_600nmPMGI-300nmPMMA_asher100W1min_+-30deg_30-60nm.PNG
    Vivien always does ashing 1' 100W before evap (etches 30nm PMMA/ min) + in situ ion milling. Works on sapphire
    10.65 Ko11:49, 6 Nov 2014Helene_Le_SueurActions
     VSsince04-2014_grid100n_600nmPMGI-300nmPMMA_asher100W1min_+-30deg_30-60nm.PNG
    Aucune description
    8.46 Ko11:49, 6 Nov 2014Helene_Le_SueurActions
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